Process of treating fullers&#39; earth.



G. L. PARSONS.

PROCESS OF TREATING FULLERS EARTH.

APPLICATION FILED AUG 29, 1906.

1 9 1 2 650), Patented. 0st. 6, 1914.

5114mm tor fidrles L par$0n s,

CHARLES L- rsasons, or bUBHAM, new mun-5313B.

rnocnss or TREATING ruLLEBs' EARTH.

Specification of Letters Patent. 4 Application filed August 29, 1908.Serial No. 332,528.

Patented Oct, 6, 1914;

To all whom it may concern.

Be it known that I, CHAnLns-L. Parsons, a citizen of the United States,residing at Durham, in the county of Straflord and State of NewHampshire, have invented certain new and useful Improvements inProcesses of Treating Fullers Earth, of which the following is aspecification.

This invention relates to a process of treating fullers earth,especially fullers earth associated with impurities, foreign matter andthe like and has particular reference to the treatment of fullers earthwhich has been employed in the refiningof edible or other oils.

' At the present time fullers earth which has been employed in thetreatment or refining of commercial oils is a waste product except inthe case of the fullers earth use in refining petroleum products, whichis purified in some degree ,by burning the com bustible materialassociated with the fullers earth residue.

As is well known, fullers earth comprises mineral matter in the form ofa clay capable of occluding or adsorbing and holding dye stufis. In usein refining oils it takes up impurities, notably coloring matters,therefrom, until rendered more or less inert by the inhibiting action ofthe selectively occluded or adsorbed oils or constituents of the oilsunder treatment. "Prior to the discovery upon whlch this invention isbased, no method was known of freeing such zeolitic material from thecoloring matters and other impurities referred to, so that it, as wellas the oil contained therein could be recovered in a condition suitablefor com mercial use.

Now I have discovered that, if fullers earth residues resulting from theuse of this material in refining oil be treated with a solvent of the'oil,such as carbon tetra chlorid and a solvent of thecoloring matterremoved from the oil in the said treatment, such as ethyl alcohol or amixture of ethyl alcohol and an acid, preferably acetic acid,

fullers earth can be recovered from the residues which is for ,allpractical purposes identical with that originally used and further thatthe oil contained in the'said residuescanberecovered in commerciallyvaluable form.

In the practice of my process in its preferred embodiment, I treat,fullers earth residues of the character before mentioned with carbontetrachlorid to remove most of the 011 present, free from excess ofcoloring matter, and follow this with a mixture of four parts by volumeof-carbon' tetrachlorid and three fourths part by volume'of ethylalcohol and one fourth part by volume of acetic acid until the coloringmatter and'any remaining oil contained in the residues are eliminatedtherefrom. The relative amounts of the said mixture and fullers earthresidues is not important, and satisfactory results may be obtained byextracting the residues with this liquid mixture in. any suitableextraction apparatus. a

The liquids containing oil and coloring matters in solutionare removedfrom the fullers earth by leaching, centrifugal action or the use of afilter press and the carbon tetrachlorid, alcohol and acetic acid areseparated .from the dissolved oil, coloring matters, etc., bydistillation. The remaining fullers earth is freed from the adheringsolvents by blowing steam or hot air through the mass and is dried andground to proper size.

In the accompanying drawings, I have shown in elevation an apparatus inwhich my process may be advantageously carried out.

In the use of this apparatus the fullers earth is placed in anextractor- 1 and the solvent allowed to gradually percolatetheretaken upthe oil or the oil'and the coloringmatter, it is drawn ofl throughvalve-controlled pipe 3 into a tank or boiler 4 where it is heated bysteam. introduced into steam coil 5.. The tank or boiler 4 may beadvantageously provided with gage glasses 6 as shown. Upon being heatedin the tank or.

boiler 4 the solvent volatilizes and passes through pipe 7 into acondensing coil 8 contained in condenser 9, where the solvent iscondensed. The solvent, upon being condensed returns to the extracter 1,through pipes 10 and 2 between which is disposed a trap 11 of the usualconstruction which serves to remove any water which may be contained inthe solvent. The solvent in the tank or boiler 4 is subjected to atemperature 5 above the boiling point of such solvent and upon itsevaporation, the oil or coloring matter and oil remains in the tank orboiler 4 and may be removed therefrom by a suitable outlet (not shown).

The fullers earth may I the extractor 1 to the action of a solvent ofthe oil and later a solvent oi the coloring matter or the fullers earthmay be subjected in the extractor A to a solvent of the oil and thecoloring matter as hereinbefore indicated. v

The oil resulting from the treatment of fullers earth residues in themanner described and the recovered fullers earth are 20 commercialproducts of sufficient value to pay for their recovery.

While I have mentioned carbon tetrachloridas the solvent of oil andethyl alcohol or better acidified ethyl alcohol as the solvent of thecoloring matter, which ll'prefer'to employ, my invention is notrestricted to the use of these two materials, as chloroform, gasolene,benzene and ether, as .well

as numerous other volatile compounds are also solvents of the oil andmay be employed. Furthermore methyl alcohol or a mixture of methyl orethyl alcohol or either withsome acid, or their reaction products withsaid acid, are solvents of the coloring matters contained in fullersearth residues and their use is contemplated as within the purview of myinvention.

While I have described the preferred embodiment of my invention ascomprising the treatment of the residues mentioned, first with a Solventof the oil and then'with r solvent of the coloring matter, my inventionis not limited thereto, as the solvents mentioned may be employedtogether in one operation although as stated, their use in two stages ispreferred.. Carbon tetrachlorid is preferably employed in the secondstage because it has the property of reducing or wholly overcoming thecombustibi'lity, of the alcohol and acetic acid and thereby reducingfire risks.' ltj may be stated in this connection that my preferredmixture which comprises: four parts by volume of carbon tetrachlorid andthree fourthsjpart of alcohol and. one fourth part acetic acidisnon-combustible and hence itsv use in the second stage oat-my processis particularlysatisfactory. If this mixture is used in the first stageof my process, the recovered oil is highly colored and notso valuable asrecoverediheitore the main part oi the-com tained coloringm-atter isextracted In some casesll have ioundthat it is not necessary to'employany acid in connection with the alcohol or other solvent or" the col:

be subjected v in inraeto ori ng matter contained in the residues inorder to completely dissolve it, but in many if not most cases thecoloring matter is not present in a form wholly soluble in the saidsolvent. By the use of an acid in connection with the solvent employedto dissolve the coloring matter the composition of the lat ter ismodified by combining with the acid and a salt results which is freelyand Wholly soluble in the solvent. Acetic acid is particularly welladapted for use with the solvent for its combination with the coloringmatters produces acetates which are very freely soluble in said solvent.Acetic acid is also preferred because it mixes easily with carbontetrachlorid and alcohol and is readily volatile. -Any other acid wouldserve to help remove the coloring matter provided the fuller-s earth wastreated with it previous tothe removal of the coloring matter or at thesame time as the treatment with alcohol.

Having thus described my invention, what I claim and desire to secure byLetters Patent, is: LA process of treating -,fullers earth residuesresulting from an oil refining process, which comprises adding to thesaid residues a solvent of the oil treated in the said process and asolvent of the coloring matter normally contained in said oil andseparating said solvents and dissolved contents from the mass. I

2. A process of treating fullers earth residues resulting from an oilrefining process Which comprlses adding to the said'residues in aselected order of succession, a solvent of oil treated in the sameprocess and a solvent of the coloring matter normally contained in saidoil and separating ms the solvents and dissolved contents from the mass.

3. A process of treating fullers earth residues resulting from an oilrefining process which comprises adding to the residues 0 a solvent ofthe oil treated in the said process and a solvent of the coloring matternormally containedin said 'oil, said first named solvent not being asolvent of the said coloringmatter,-- and separating said solvents 115and dissolved contents from the mass 4. A process oftreating fullersearth residues resulting from an oil refining process, which comprisestreating the same with a solvent of the oil treated in the said process120 and-a solvent of coloring matter normally contained in said oil,said first namedsolvehtnot being a solvent of the said coloring-matter,whereby said oil and coloring matter are dissolved, removing the saidsol- 125 events from the mass and separating the dissolved oil from itssolvent.

' 5.- A process of treating fullers earth residues resulting from anoil. refining process, which comprises treating the same in a 130selected order of succession with a solvent of the oil treated in thesaid process and a solvent of the coloring matter. normally tents fromthe mass. {p

7 ,A process of treating fullers earth resimixture and diss contained insaid oil, said first named solvent not being a solvent of the saidcoloring matter, whereby said oil and coloring matter aredissolved,removing the said solvents and dissolved contents from the mass andseparating the dissolved oilfrom its solvent and the dissolved coloringmatter from its. solvent. 7

6. A process of treating fullers earth residues resulting from an oilrefining roce'ss, which comprises adding to said residues a solvent ofthe oil treated in said process, to which solvent an acid has been addedand separating said solvent and dissolved condue s resulting from anoil-refining process, whlch comprlses first treating the same with asolvent of the oil treated in said process,-

said solvent notbeing a solvent of the colormg matter normally containedin said oil, then treating the said residues with a solvent of thecoloring matter normally contamed 111 said oil and separating the saidlved contents from the mass.

- solvents.

. 9. A- process of treating fullers? earth resi- 4 8. A process oftreating fullers earth residues resulting from an oil refining process,which comprises treating the same w1th car bon tetrachlorid andacidified alcohol wherei by said oil and coloring matter are dissolved,

removing the said materials from the mass and separatmg the dissolvedoil and dissolved coloring matter from their respective dues resultingfrom an oil refining process, WhlCll comprises first treating the samewith carbon tetrachlorid, then removing the said carbon tetrachlorid anddissolved contents, next treating the residue with acidified alcohol,then removing the said alcohol and .dissolved contents; and finallyseparating the dissolved oil and coloring matter from their respectivesolvents.

-10. A process .of treating fullers earth residues, resulting from oilrefining processes, which comprises removing the main part of the oiltherefrom with a solvent of the oil, then treating the residue with amixture containing approximately four parts by volume of carbontetrachlorid, three fourths part by volume of 'alcoholand one fourthpart by volume, of acetic acid until the oil and coloring mattercontained in the mass treated are dissolved, separating the alcohol andacid from the'mass and -rec0vering the carbon tetrachlorid and alcoholand acid from the dissolved oil and' coloring matter. H

11. A process of treating fullers. earth residues, I resulting from oilrefining proc 65 esses, which comprises first removing .the greaterportion of the oil by means ofa solvent thereofwhich is not asolvent ofthe coloring matter normally contained in the said oil, treating theresidue with acid1- fied alcohol untilthe coloring matter contained inthe mass is dissolved, sep arating' saltsoluble in said solvent,substantially as dec'ribed.

In testimony whereof I affix my slgnature in presence of two Witnesses.

CHARLES L. PARSONS. Witnesses: CHAS. WENTWOBTH H. H. SMALL;-

